Spectroscopic and Structural Characterization

The scopes outlined above limit the purpose of this chapter, which will not cover (1) the transition metal complexation by protonated or functionalized forms of calix[4]arenes (2) the metalation of calix[4]arenes using non-transition metals and (3) chemical curiosities derived from the metalation of calix[4]arenes (some recent reviews cover these areas very well).1 In addition, the authors have been particularly careful to report only those compounds which have a well-established synthesis and a full spectroscopic and structural characterization. 

When Y is a highly nucleophilic anion like F, Cl, CN, or C6F5C02", the organoxenon compound RXeY has covalent character (6). Although the chemical, spectroscopic, and structural characterizations of these compounds are outside the scope of this review, a several sets of typical NMR spectroscopic data for covalent pentafluorophenylxenon derivatives C6F5XeR (R = F, Cl, C6F5) are included in Tables I and II for comparison. 

In this paper author reported the reactivity of newly synthesized Co(III)-nitrosyls complexes with superoxide radical to follow nitric oxide dioxygenation. Two new Co(III)-nitrosyl complexes bearing N-tetramethylated cyclam (TMC) ligands, [(12-TMC)-Com(NO)]2+ (1) and [(13-TMC)Coin(NO)]2+ (2), were synthesized via [(TMC)Con(CH3CN)]2+ + NO(g) reactions. Spectroscopic and structural characterization showed that these compounds bind the nitrosyl moiety in a bent end-on fashion. Complexes 1 and 2 reacted with K02/2.2.2-ciyptand to produce [(12-TMC)Con(N02)]+ (3) and [(13-TMC)Con(N02)]+ (4), respectively these possess 0,0 -chelated nitrito ligands. 

H. Willner, and F. Aubke, Homoleptic Metal Carbonyl Cations of the Electron-rich Metals Their Generation in Superacidic Media Together with Their Spectroscopic and Structural Characterization, Angew. Chem. Int. Ed. Engl. 36, 2402-2425 (1997). 

Takani, M., Yajima, T., Masuda, H. Yamauchi, O. (2002). Spectroscopic and structural characterization of copper(II) and palladium(II) complexes of a lichen substance usnic acid and its derivatives. Possible forms of environmental metals retained in lichens. Journal of Inorganic Biochemistry, 91, 139-50. 

Cp-amido titanium complexes containing different amido substituents including amino functionalities (Scheme 310) have been prepared by the appropriate synthetic route and spectroscopically and structurally characterized. In some cases, intramolecular coordination of the amino-nitrogen atom is observed according to the X-ray diffraction data. These complexes when activated with MAO are catalytically active for ethylene polymerization.753... 

Spectroscopic and Structural Characterization 3.4.3.1 Pyrolysis-Mass Spectrometry... 

RhCl(Cp )(Tpx)] have been synthesized by the reaction of the appropriate [RhCl2(Cp )]2 with K(Tpx) (Tp = Tp or Tp ). These complexes have been spectroscopically and structurally characterized. 

E. C. Zampronio and H. P. Oliveira, Synthesis, spectroscopic and structural characterization of poly-o-methoxyaniline and poly-o-methylanihne intercalated into layered vanadyl phosphate. Mater. Res. Bull, 39, 1525-1538 (2004). 

Studies of coordination chemistry in the gas phase include spectroscopic and structural characterizations, similar to information gleaned in condensed phase work. Somewhat uniquely, the gas phase also allows the characterization of unsaturated coordination complexes and the measurement of the thermochemistry of metal ligand bonds. This latter topic will be the focus of the present article. In particular, trends in the thermochemistry will be discussed, including comparisons among the bond dissociation energies (BDEs) for a variety of metals, ligands, and numbers of coordinated ligands. Most of the work discussed here involves the +1 oxidation state of all metals, an unusual oxidation state for many metals in the condensed phase except for... 

Among the proteins that accommodate interconvertible [3Fe-4S]/[M3Fe-4S] clusters, the ferredoxin from Pyrococcus furiosus (P.f Fd) has received most attention in terms of spectroscopic and structural characterization [74,75,77,78], The [3Fe-4S] cluster occupies a binding domain resembling that of typical [4Fe-4S] clusters except that one of the cysteines (the central one in the triad) is replaced by aspartate (D), i.e., the binding motif is Cys-Xaa-Xaa-Axp-Xaa-Xaa-... 

The hereto unknown and very sensitive l,2-bis-(5-azido-17f-tetrazolyl)ethane has been prepared, spectroscopically and structurally characterized (Figure 13.11 and Scheme 13.18). This substance is highly explosive, as the preliminary sensitivity data demonstrate (friction <5N, impact >0.15 J). The synthesis is achieved in four steps all with good yields ranging from 40-80%, starting with triethyl orthoformate, ethylene diamine and sodium azide. The introduction of the azide group at the tetrazole moiety occurs at the last step and therefore it can be regarded as a very safe synthesis to prepare a bis-tetrazolyl alkane. 

Kaliva M, Kyriakakis E, Gabriel C, Raptopoulou CP, Tarzis A, Tuchangues JP, Salifoglou A (2006) Synthesis isolation, spectroscopic and structural characterization of a new pH complex structural variant from the aqueous vanadium(V)-peroxy-citrate ternary system. Inorg Chim Acta 359 4535 548... 

Zhou ZH, Zhang H, Jiang YQ, Lin DH, Wan HL, Tsai KR (1999) Complexation between vanadium(V) and citrate spectroscopic and structural characterization of a dinuclear vanadium(V) complex. Transit Met Chem 24 605-609... 

Zhou ZH, Wan H.l Tsai KR (2000) Syntheses and spectroscopic and structural characterization of molybdenum(VI) citrate monomeric raceme and dimer, K [Mo03(cit)] 2H2O and KJ(Mo02)20(Hcit)2l 4H2O. Inorg Chem 39 59-64... 

Matzapetakis M, Raptopoulou CP, Tsohos A, Papaefthymiou V, MoonN, Salifoglou A(1998) Synthesis, spectroscopic and structural characterization of the first mononuclear, water soluble iron-citrate complex. J Am Chem Soc 120 13266-13267... 

The synthesis, spectroscopic and structural characterization of bromo-boryl complexes have been reported, and they have been shown to be versatile substrates for the synthesis of both asymmetric boryl complexes and bridging borylene complexes, for example, (r7 -G5H4R)Fe(GO)2 2(M"EMe) where R = H 82 and R = Me 83, via substitution chemistry with retention of the metal-boron bond. " Gomplexes 82 and 83 are the first reported examples of structurally characterized bridging borylene complexes without a supporting M-M bond. 

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